固相萃取-气相色谱-串联质谱法同时测定人体尿液中4种有机磷农药代谢物

建立了同时测定尿液中4种有机磷类农药代谢物的气相色谱/串联质谱分析方法。尿液样品以WCX固相萃取柱富集提取,乙酸乙酯-乙腈（70∶30,V/V）再萃取,浓缩干燥,甲苯溶解,N-叔丁基二甲基甲硅烷基-N-甲基三氟乙酰胺衍生化。采用HP-5MS色谱柱（30 m×0.25 mm×0.25μm）程序升温分离,串联质谱多反应检测,内标法定量。通过比较尿样中代谢物在不同萃取溶剂、固相萃取柱及p H值洗脱液等条件下的回收率,优化了前处理方法。在0.2~200μg/L范围内,4种代谢物峰面积与内标峰面积的比值与质量浓度的线性关系良好（R^2≥0.992）,方法检出限为0.083~0.667μg/L,定量限为0...

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Bibliographic Details
Published in分析化学 Vol. 44; no. 5; pp. 723 - 730
Main Author 黄梦莹 王娜 郭欣妍 邱盼子 汤卫国 张尊建
Format Journal Article
LanguageChinese
Published 环境保护部南京环境科学研究所,南京210042 2016
金陵药业股份有限公司,南京210009%环境保护部南京环境科学研究所,南京,210042%金陵药业股份有限公司,南京,210009%中国药科大学药物质量与安全预警教育部重点实验室,南京,210009
中国药科大学药物质量与安全预警教育部重点实验室,南京210009
Subjects
固相萃取
尿液
有机磷农药代谢物
气相色谱-串联质谱
Urine
Solid phase extraction
Organophosphorus pesticides metabolites
尿液
Gas chromatography-tandem mass spectrometry
固相萃取
有机磷农药代谢物
气相色谱-串联质谱
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ISSN0253-3820
DOI10.11895/j.issn.0253-3820.150932

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Summary:建立了同时测定尿液中4种有机磷类农药代谢物的气相色谱/串联质谱分析方法。尿液样品以WCX固相萃取柱富集提取,乙酸乙酯-乙腈（70∶30,V/V）再萃取,浓缩干燥,甲苯溶解,N-叔丁基二甲基甲硅烷基-N-甲基三氟乙酰胺衍生化。采用HP-5MS色谱柱（30 m×0.25 mm×0.25μm）程序升温分离,串联质谱多反应检测,内标法定量。通过比较尿样中代谢物在不同萃取溶剂、固相萃取柱及p H值洗脱液等条件下的回收率,优化了前处理方法。在0.2~200μg/L范围内,4种代谢物峰面积与内标峰面积的比值与质量浓度的线性关系良好（R^2≥0.992）,方法检出限为0.083~0.667μg/L,定量限为0.2~2.0μg/L,平均回收率为54.1%~68.6%,相对标准偏差均小于8.5%（n=6）。本方法稳定、可靠,分析时间短,不需要使用大量有机溶剂,可同时处理大批量样品,适用于人群有机磷类农药暴露情况的评估。
Bibliography:A method for quantifying four urinary metabolites of organophosphorus pesticides using gas chromatography-tandem mass spectrometry （GC-MS/MS） was developed. The metabolites were extracted and enriched from urine samples with WCX solid phase extraction （ SPE ） cartridges, followed by liquid-liquid extraction with ethyl acetate-acetonitrile （70： 30, V/V）. The analytes were chemically derivatized with N-tert- butyldimethylsilyl-N-methyhrifluoroacetamide after the derivatives were concentrated by drying and dissolved in phenylmethane. The separation was performed on a HP-SMS capillary column （30 rex0.25 minx0.25 μm） with temperature programming and the detection was performed in multiple reaction monitoring （MRM） mode using GC-MS/MS. The internal standard method was used for quantification. The extraction solvents, types of SPE cartridges and eluents were optimized by comparing the sample recoveries under different conditions. The result showed that the calibration curves of four metabolites were linear in the ra
ISSN:0253-3820
DOI:10.11895/j.issn.0253-3820.150932